Process of making hardened fat and the like.



O. ELLIS.

PROCESS OF MAKING HARDENED FAT AND THE LIKE.

APPLICATION FILED DEC. 21, 1912.

1,059,720. P n d Apr. 22, 1913.

In V611 tor.-

rnocnss or MAKING nnannnnn FAT arm ran M.

Specification 0! Letters Potent.

' Patented Apr. bib, 1913.

Application filed December 21, 1912. serial 1%. 737,942.

hydrogenating oily material and the like,

containing. unsaturated bodies, and relates .in particular to the treatment of a body of oil with hydrogen or a hydrogen-containing gaseous medium, involving passage of the gas preferabl in relatively finebubbles through said of oil; all as more fully 'l'iereinafter described and claimed.

' It has been proposed to hydrogenate oil bypassing a strong current of hydrogen therethrough in the presence ot a very fineiy divided catalyzer such asmetallic nickel and the like, this having been advanced among others by Nor-maxim, Eng. Patent No. 1515, of 1905; Also it has been proposed to make use of pressure in accelerating the rate of hydrox'ration as has been repeatedly advancflby Ip'atiefi' Day and others. In the seat invention 1- make use prefmbly o two very common expedient. namely that of stirring'a liquid by means a? a gas passing through it and the use of pros sure to accelerate reactions between liquids:

and wees-, but. I embody with these aforesaid oomniorr cnpedients? acertain novel method of operation asiwill hereinafter be desciibedt heretotore stated (Journalof mesa eiiotamimzzn wayne1e, page LL62) n ot'appeairneedfokto agitate the cetelyaerto the extent heretofore supposcdt- Gentrary to the-opinion entertained 7 b mayjhereqppea s to-beno occasion to agitate-jabs catalyzes primarily for the rposeoff/contacting. it with hydrogen. nee

the oatalyzer iswetted with the-01lthere can Ion or locally actual contact with the gas ydrogen reaches the catalyzer seem mg'ly' only through-solution; in the oil. The forces oi: adhesion effectually seal the cata* 1-year surface from the gas and no'measure et by ordinary mixin I will dislodge the film oi oil. 0 course agitation seeuresthe-ra pid replacement at more saturated by. lesssaturated rti'ons' of the oil-, but this'r-eplacem'ent un or certain con p diticnsmay proceed.jiust as rapidly, simply to the required apparatus The eflect of agitation is in fact =1: rded by some as undesirable just as in the mam-1- facture' of soda water it is found that whipping of the Water contained in the has a tendency to drive the gas from solution,

whereas gentle agitation under pressure offacts rapid saturation. In the same manner violent agitation of the oil with hydr gas, such as is sometimes resorted to, tends to whip the gas tron) the oil and does not permit of itsefiective solution therein-arid in consequence of the fact that the gas can get to the catalyze? substantially only by way of the oil it follows that the oi hydrogenation or the desirable tom era:

ture required cannottake placeefi'ective y}.

By the present invention I may subjebt the oil to a pressure which is frequentlyvariable in amount, although the variation is preferably slight and definite and 025 a positive nature. To this end- I may a body of oil to an atmosphere of. and cause a portion of the oil to pass f erably under a substantial pressure theme an injector in such a manner that the hydro; gen gas is drawninto contact with the" oil so that without the formation of a ertul spray or violent mechanical a 'tatien hydrogen is brought intosolu-tion by this oil gree- During the period of induction the 011 and gas are subjected maomentarily to reduced pressure which causes the elimination moroor less of ti or "microscopic bubbles of hydra whii; become attracted to the particles'oif'catalyzer and adhere to same leyadhesiye forces until absorbed through the filfn of oil by the ester lyzer' and then given back to-t'heoilas hydrogen. ThusI eferabl con; ditions suchthat t e artic es 9. eatalyaer carry a zone of near y saturated ta even \supersaturated solution -o,hydrogen in the oil. aroundabout each particle. p

The catalyzer which I may employ is tha*t of SabatieJ onsisting of metallic; m w

- supported on a carrier of pumice or o her similar granular material including I earth and the like'and repari'ngthismaterial I may simply emp 0y the recess o t- Sabatier,- namely that of wetting. t e. fuller's" earthor pumice with nearly saturated solu tion of nickel nitrate, dryin igniting. and then reducing in a current 0 hydrogen; or

I may employ the following method of preparing the catalyzer whichconsists in taking thematerial' prepared in the foregoing man ner and after reduction while still hot e rposing to air to reoxidize and then reducing a second time so as to secure a doubly reduced material which contains a larger proportion of metallic nickel than is possible to obtain by a single reduction, especiallyat the working temperatures desired for catalyzer reduction, namely 300 to 350 C. I do not, however, find the use of highly porous supporting bodies as desirable as thos which are denserl Pumice and keiselguhr are so porous that they absorb vast quantities of the nickel solution in to the interior pores and once in there this is sealed by the oil from further activity. Thus probably onehalf of the nickel used is rendered ineffective or inefficient. For practical operation under such circumstances such inert carriers are therefore obviously often undesirable. Charcoal material and the like, of an active character, may be used in carrying out the process of the present invention. Charcoal has the property of absorbing hydrogen and often exhibits desirable catalytic properties.

In carrying out my process I make use of the following arrangement of apparatus: The oil is placed in a hydrogenating tank which is preferably heated by a steam coil and hydrogen is introduced into this tank under any suitable pressure, it being desirable to heat the oil and blow hydrogen through it for a short time to remove moisture and air. Catalyzer is prepared in a separatechamber consisting, for example, of a drum which is caused to rotate in a receptacle heated to 300 or 350 C. while hydrogen is passed over same. The drum of catalyzer is then tightly closed, carried to the hydrogenation tank, screwed into a threaded opening in the tank and the contents are allowed to fall into the receptacle without contact with the air, as even momene tary exposure to air is almost fatal of good results. Oil is then heated in the hydrogenation tank and a portion passed in cyclic fashion through the injectors so as to introduce hydrogen from the top of the tank into the bottom of the tank and the hydrogen entering in this way at the bottom of the tank is so mingled with the oil that relatively fine bubbles of the oil are formed particularly conducive to rapid absorption. In the inductor it is desirable to avoid the formation of spray and the stream of oil passing through inductor should therefore be as nearly solid or integral as possible so as to avoid separating the'gas in solution in the oil.

It is desirable oftentimes to withdraw from the hydrogenation tank a slow stream of hydrogen in order to gradually relieve the gas of its spent portion; fresh gas, of course, being fed into the apparatus. The spent gas is well suited for reducing catalyzer, especially if it is somewhat purified.

The purified spent gas may be used for making the first reduction ofthe catalyzer and the final reduction may be made with pure hydrogen.

The accompanying drawing shows in vertical section apparatus suited for carrying out the present invention.

In the drawing 1 is a treating receptacle or tank having the steam heating coils 2 and oil inlet and outlet 3.

4 is a draw off at the bottom of the conical base.

5 is an inlet for hydrogen gas.

6 is a gas exit.

7 is a pump placed below the oil level 18 and having an inlet 8. p

9 is a pipe leading from the pump 7 to the injector 10 having the exit pipe 11 and vgas inlets 12.

13 is a thermometer and 14 a pressure gage. 15 is a catalyzer container having the valves 16 and 17.

In the operation of the foregoing somewhat diagrammatically shown apparatus,

hot or cold oil is placed in the tank to fill same to about the level indicated. The temperature is raised or maintained at about 300 F. and a quantity of hydrogen or a hydrogen containing gas is entered at 5 to flush out all air from the tank and appurtenances. To aid this, the pump 7 is put in operation. When the air has been removed a charge of catalyzer contained in the capsule or container 15 is entered, the pump 7 set in motion or continued in motion and hydrogen or a hydrogen containing gas passed into the receptacle, to replace the portions absorbed or to create any suitable pressure.

While I do not find it necessary or desirable with the present apparatusto use the high pressures employed by Ipatieff, I may employ pressures of 2 or 3 atmospheres or so which has a tendency to steady the oil stream passing through the inductor. The precise operation of the inductor is of importance. Oil carrying catalyzer is segregated or withdrawn from the main body of pool and the former to, in the course of time, again pass through the inductor via the pump 7 No powerful circulation of the oil is requlred and the preferably gentle flow of oil and gas along the cyclic path thus created aflords full opportunity for solution of gas in the oil without danger of whipping out of the oil in a not readily available formthe dissolved gas content. Furthermore, the decrease in pressure at the time of induction apparently tends to cause microscopic bubbles of hydrogen to collect on the particles of catalyzer and thus to-be taken up readily in contrast with the dislodging effect caused by spraying or whipping the oil under certain circumstances.

By treatment of unsaturated fats and oils, such as tallow, oleostearin, cotton, c0rn, rape, peanut, castor, linseed, Chinese Wood, fish, whale and similar oils with hydrogen and the like in the presence of a catalyzer such as nickel or palladium, a hardening of the oil results through formation ofstearins and other solid bodies. Certain waxes may be hardened in a similar manner. By the use of oxygen and hydrogen the hydroxy compounds may be secured.

, To recapitulate, the present invention relates to the process of treating oily material and the like containin bodies which comprises confinlng a body of said material, admixed with a catalyzer, in juxtaposition to a hydrogen-containing gaseous medium, in segregating from said body portions thereof, as by continuously impelling (withdrawing) from said body a stream of oil, in passing such portions or said stream through some portion of said gaseous medium whereby entrainment of some portion of the latter occurs, and in causing said segregated oil and gas preferably in the form of a stream to enter said body of oil beneath the surface thereof preferably in a continuous manner; whereby said gas is disseminated through said body of oil, and saturation of at least a portion of said unsaturated bodies is effected.

unsaturated What I claim is:

1,. The process of treating oily material and the like containing unsaturated bodies which comprises confining a body of said material, admixed with a catalyzer, in juxtaposition to a hydrogen-containing gaseous medium, in withdrawing from said body portions thereof, in passing such portions through some portion of said gaseous medium; whereby entrainment of some portion of the latter occurs, and in causing the with drawn oil-and entrained gas to'enter said body of oil beneath the surface thereof; whereby saturation of at leasta portion of said unsaturated bodies is effected.

2. The process of treating oily material and the like containing unsaturated bodies which comprises confining a body of said material, admitted with catalyzer, in juxtaposition to a hydrogen-containing gaseous medium under pressure, in continuously withdrawing from said body portions there of, in passing such portions through some portion of said gaseous medium; whereby entrainment of some portion of the latter occurs, and in causing the withdrawn oil and entrained gas to enter said body of oil at a. point well beneath the surface thereof; whereby saturation of at least a portion of said unsaturated bodies is effected.

Signed at Montclair in: the county of Essex and State of New Jersey this 12th day of December A. D. 1912.

OARLETON ELLIS.

, WVitnesses:

B. M. ELLIS, F. CARBU'rr. 

